Potassium Iodide → HCID 13078406、化合物

HRID 223260ノート

反応式

HRID 223260 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7]([CH:10]3[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]3)[C:6]=2[CH:16]=1.Cl[CH2:18][CH2:19][CH2:20][N:21]1[C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=2[NH:23][C:22]1=[O:30].C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>CC(CC(=O)C)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7]([CH:10]3[CH2:11][CH2:12][N:13]([CH2:18][CH2:19][CH2:20][N:21]4[C:25]5[CH:26]=[CH:27][CH:28]=[CH:29][C:24]=5[NH:23][C:22]4=[O:30])[CH2:14][CH2:15]3)[C:6]=2[CH:16]=1

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 18104191-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-oneHCID 27947555-Fluoro-3-(4-piperidinyl)-1,2-benzisoxazole

生成物 1

HCID 13078406HCID 13078406、化合物収率 35.8%

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

A mixture of 3.9 g of 5-fluoro-3-(4-piperidyl)-1,2-benzisoxazole, 3.8 g of 1-(3-chloropropyl)-1,3-dihydro-2H-benzimidazol-2-one, 2.7 g of sodium carbonate, a few crystals of potassium iodide and 140 ml of 2-methyl-4-pentanone was stirred and was heated under reflux under nitrogen for 8 hrs. After stirring at ambient temperature for 12 hrs, the mixture was filtered and the filter cake was stirred with 200 ml of water. The solid was collected and dried. Recrystallization from methanol-dimethylformamide-water gave 2.5 g (35.8%) of product. The product was combined with 1.0 g of that from another run to yield a total of 3.5 g of product, mp 202°-204°.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux under nitrogen for 8 hrs
  3. filtrationthe mixture was filtered
  4. stirringthe filter cake was stirred with 200 ml of water
  5. customThe solid was collected
  6. customdried
  7. customRecrystallization from methanol-dimethylformamide-water

出典と根拠

ORDレコード
ord-8e1307a36c514b7da7d1b2f7684cdf0d
出典データセット
uspto-grants-1982_10
特許番号
US04352811

反応ノート

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